Process for the manufacture of trinitrotoluene.



FEBDINANDO QUARTIERI, OF MILAN, ITALY.

PROCESS FOR THE MANUFACTURE OF TRINITROTOLUENE.

No Drawing.

To all whom it may concern:

Be it known that I, FERDINANDO QUAR- TIERI, engineer, subject of theKing of Italy, resident of Milan, in the Kingdom of Italy, N o. 17 ViaPrincipe Umberto, have invented new and useful Improvements in Processesfor the Manufacture of Trinitrotoluene, of which the following is aspecification.

In the ordinary process of manufacturing trinitrotoluene, toluene isused as raw material and by suitable nitrations it is made intomonomtro-, then into dinitro-, and finally into trinitrotoluene, or themononitro product is transformed directly into trinitro-toluene, or thetoluene may be transformed directly into dinitr -toluene and thereuponinto trinitrotoluene. In all these various processes there is thedrawback of an abundant formation of a liquid product which, if notremoved, gives rise to an impure trinitrotoluene which must becrystallized from alcohol or other solvents in order to obtain it at thedegree of purity required for the preparation of explosives;

According to the present invention the intermediate solid productsobtained in nitrating toluene, such as impure or crude soliddinitrotoluene, for example, are submitted to a partial and fractionalliquefaction, whereby pure dinitrotoluene and a liquid containingimpurities are obtained. The pure dinitrotoluene thus separated is thenheated gradually to 110 C. by addition of a nitric sulfuric mixture(containing from 20 to 30% of nitric acid) in the pro portion of from 4.to 5 parts by weight of the mixture to one part by weight ofdinitrotoluene. By slowly cooling the mass thus obtained, abundantcrystallization of pure trinitrotoluene takes place which is washed withwater and then melted in a vacuum to eliminate volatile impurities suchas the acids. A pure product is thus obtained which after beinggranulated and dried, has an extremely high degree of Specification ofLetters Patent.

Patented Sept. 25, 1917.

Application filed August 31, 1914. Serial N 0. 859,493.

1. In the manufacture of trinitrotoluene,

the process which comprises nitrating toluene, treating the solidintermediate products of the nitration to partially or fractionallyliquefy the same and thereby to separate liquid intermediate nitrationproducts there- 'from, further nitrating the liquid intermediatenitration products thus separated, and purifying the resultant finalproduct by melting and filtration, and by heating in a vacuum.

2. In the manufacture of trinitrotoluene, the process which comprisesnitrating toluene, partially solid intermediate products formed in thenitration, and separating and further nitratin the liquid intermediateproducts thus 0 tained.

3. In the manufacture of trinitrotoluene, the process which comprisesnitrating toluene. partially or fractionally liquefying solidintermediate products formed in "the nitration. separating the resultantliquid intermediate products from the remaining solid intermediateproducts, and further nitrating both the liquid and solid intermediateproducts thus separated.

In testimony whereof I hereunto afiix my signature in the presence oftwo witnesses.

FERDINANDO QUARTIERI.

Witnesses:

B. CARLO TALVO'ITI, LYLE RoBB.

or fractionally liquefying,

